CN111960821A - Microwave dielectric ceramic material and preparation method and application thereof - Google Patents
Microwave dielectric ceramic material and preparation method and application thereof Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 39
- 239000000843 powder Substances 0.000 claims abstract description 31
- 238000000498 ball milling Methods 0.000 claims abstract description 26
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 17
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 17
- 239000000126 substance Substances 0.000 claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims description 24
- 238000005245 sintering Methods 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 22
- 239000002002 slurry Substances 0.000 claims description 22
- 238000001035 drying Methods 0.000 claims description 16
- 238000007873 sieving Methods 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 14
- 239000004575 stone Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000011230 binding agent Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 6
- 229910000018 strontium carbonate Inorganic materials 0.000 claims description 6
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 claims description 6
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000005469 granulation Methods 0.000 abstract description 5
- 230000003179 granulation Effects 0.000 abstract description 5
- 239000000919 ceramic Substances 0.000 description 24
- 238000000227 grinding Methods 0.000 description 8
- 239000008213 purified water Substances 0.000 description 8
- 239000013078 crystal Substances 0.000 description 5
- 239000007795 chemical reaction product Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000007599 discharging Methods 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000005498 polishing Methods 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000006104 solid solution Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000004891 communication Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000008054 signal transmission Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
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Abstract
The invention discloses a microwave dielectric ceramic material and a preparation method and application thereof, wherein the microwave dielectric ceramic material comprises the following chemical components: 0.6CaxSr1‑xTa2O6‑0.4LaAlO3X is 0.6 or more and 0.9 or less; preparation: LaAlO is added3And CaxSr1‑ xTa2O6(x is 0.6-0.9) is used as a raw material and is proportioned according to the stoichiometric ratio of the chemical components, ball milling is carried out, the ball milled powder is dried and sieved, then polyvinyl alcohol aqueous solution is added for granulation, and the raw blank is pressed after being ground and sieved and then sintered at 1440 ℃ 1460 ℃ to prepare the material; and the application of the microwave dielectric ceramic material in the preparation of microwave devices; the microwave dielectric ceramic material has excellent Q f value, proper dielectric constant and near zeroThe temperature coefficient of the resonant frequency meets the use requirement under the microwave condition.
Description
Technical Field
The invention belongs to the technical field of electronic information functional materials and devices, and particularly relates to a microwave dielectric ceramic with medium and low dielectric constant, high quality factor Qxf and resonance frequency temperature coefficient tau f close to zero, a preparation method and application thereof, which can be used for manufacturing microwave devices such as dielectric resonators, filters and the like and applied to the communication field.
Background
The fifth generation (5G) communication will become the mainstream wireless protocol in the fields of mobile phones, WIFI, global positioning systems, intelligent transportation systems, internet of things and the like in the next 10 years. According to the regulations of the world wireless society, the final working frequency band allocated for 5G is 24-30GHz or 60-70 GHz, and the delay time of signal transmission is less than 1 ms. Unlike 2G/3G/4G mobile communication, the carrier frequency of 5G is extended to the millimeter wave band, which has a great influence on the development of microwave dielectric ceramics. Since the delay time is proportional to the square root of the dielectric constant (r), the propagation speed of a radio signal can be increased by using a dielectric with a low r. In addition, a high quality factor (Q × f) is required to reduce energy loss, and a temperature coefficient of the resonance frequency (τ f) is also required to be almost zero to maintain operation stability.
Disclosure of Invention
The invention aims to overcome one or more defects in the prior art and provide a novel microwave dielectric ceramic material which has an excellent Q f value, a proper dielectric constant and a near-zero temperature coefficient of resonant frequency and meets the use requirement under the microwave condition.
The invention also provides a preparation method of the microwave dielectric ceramic material.
The invention also provides an application of the microwave dielectric ceramic material in preparation of microwave devices.
In order to achieve the purpose, the invention adopts a technical scheme that:
a microwave dielectric ceramic material comprises the following chemical components: 0.6CaxSr1-xTa2O6-0.4LaAlO3X is 0 or more6 and 0.9 or less.
According to some preferred and specific aspects of the present invention, x is greater than or equal to 0.8 and less than or equal to 0.9.
According to some preferred aspects of the present invention, the sintering temperature of the microwave dielectric ceramic material is 1440-1460 ℃.
According to the invention, the dielectric constant r of the microwave dielectric ceramic material is 19.43-25.22, the quality factor Qxf is 100232-124564 GHz, and the temperature coefficient tau f of the resonance frequency is-16.3 to-1.5 ppm/DEG C.
The invention provides another technical scheme that: the preparation method of the microwave dielectric ceramic material comprises the following steps:
(1) with SrCO3、CaCO3And Ta2O5As a raw material, in accordance with CaxSr1-xTa2O6The formula is prepared according to the stoichiometric ratio of (A), x is more than or equal to 0.6 and less than or equal to 0.9;
(2) performing wet ball milling on the material prepared in the step (1) to obtain slurry-like material;
(3) drying the slurry-like material prepared in the step (2) to constant weight to obtain a dry mixture;
(4) sieving the mixture prepared in the step (3), and pre-sintering at 1110-1180 ℃ to prepare CaxSr1- xTa2O6Powder, x is more than or equal to 0.6 and less than or equal to 0.9;
(5) LaAlO is added according to the stoichiometric ratio3Adding the Ca prepared in the step (4)xSr1-xTa2O6Performing wet ball milling on the powder to obtain premixed slurry;
(6) drying the premixed material prepared in the step (5) to constant weight to obtain premixed powder;
(7) sieving the premixed powder in the step (6), and mixing the sieved material with a binder to prepare a green body;
(8) placing the green body prepared in the step (7) in a high-temperature furnace, heating to 580-620 ℃ at the speed of 2.5-3.5 ℃/min, and preserving heat for 2.5-3.5 h;
(9) will pass through step (8)Sintering the processed green body at 1440-1460 ℃ to prepare the microwave dielectric ceramic material with the following chemical components: 0.6CaxSr1-xTa2O6-0.4LaAlO3And x is 0.6 or more and 0.9 or less.
According to some preferred and specific aspects of the present invention, in the step (2), the wet ball milling is performed by using the material prepared in the step (1), ball mill stone and water in a mass ratio of 1: 2 to 4: 1.0 to 1.4.
According to some preferred and specific aspects of the present invention, in the step (2) and the step (5), the ball mill used for the wet ball milling is a planetary ball mill, and the rotation speed is set to be 110r/min to 180 r/min.
According to some preferred aspects of the invention, in the step (7), the binder is polyvinyl alcohol, the polyvinyl alcohol is added in the form of an aqueous solution of polyvinyl alcohol, and the addition amount of the polyvinyl alcohol is 2-8% of the material discharged from the sieve of the premixed powder in percentage by mass.
According to some preferred and specific aspects of the present invention, in the step (9), the sintering treatment includes: heating to 1440-1460 ℃ at a speed of 2.5-3.5 ℃/min.
The invention provides another technical scheme that: an application of the microwave dielectric ceramic material in the preparation of microwave devices.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
the invention innovatively provides a novel microwave dielectric ceramic material which is prepared from CaxSr1-xTa2O6LaAlO is used as the main crystal phase material3The doped material is obtained through continuous practice and exploration, and the inventor finds that when the relative content of the doped material and the relative content of the doped material are respectively limited to 0.6 and 0.4; and when x is more than or equal to 0.6 and less than or equal to 0.9, the microwave dielectric ceramic material can be sintered and molded at a lower sintering temperature (1440-1460 ℃), particularly a more ideal Qxf value, a nearly zero tau f value and a proper dielectric constant can be obtained, the use requirements under microwave conditions can be met, and meanwhile, the preparation method is simpler and is easy to implement.
Detailed Description
The above-described scheme is further illustrated below with reference to specific examples; it is to be understood that these embodiments are provided to illustrate the general principles, essential features and advantages of the present invention, and the present invention is not limited in scope by the following embodiments; the implementation conditions used in the examples can be further adjusted according to specific requirements, and the implementation conditions not indicated are generally the conditions in routine experiments.
Not specifically illustrated in the following examples, all starting materials are commercially available or prepared by methods conventional in the art.
Example 1
This example provides a microwave dielectric ceramic material with a chemical composition of 0.6CaxSr1-xTa2O6-0.4LaAlO3(x ═ 0.6), the preparation method comprising the steps of:
(1) preparing materials: raw material SrCO3、CaCO3And Ta2O5As a raw material, in accordance with CaxSr1-xTa2O6(x is 0.6) in a stoichiometric ratio;
(2) mixing materials: mixing the materials obtained by proportioning, ball milling stones and purified water according to the proportion of 1: 3: 1.2, putting the mixture into a ball mill for wet ball milling (the rotating speed is about 150r/min), wherein the ball milling time is 20 hours, and obtaining slurry raw materials;
(3) drying: putting the slurry raw material in the step (2) into an oven to be dried to constant weight to obtain a dry mixture;
(4) pre-burning: sieving the mixture obtained in the step (3) with a 80-mesh sieve for dispersion, and then placing the mixture into a high-temperature furnace for presintering for 4 hours at the presintering temperature of 1150 ℃ to obtain CaxSr1-xTa2O6(x ═ 0.6) powder;
(5) ball milling: adding the Ca of the step (4) according to the stoichiometric ratioxSr1-xTa2O6Adding pure LaAlO into (x is 0.6) powder3Adding purified water, and grinding in a ball mill for 10h to form premixed slurry;
(6) drying: placing the premixed slurry obtained in the step (5) in an oven, and drying at 60 ℃ to constant weight to obtain premixed powder;
(7) and (3) granulation: sieving the premixed slurry obtained in the step (6) by using a 60-mesh standard sieve, adding a polyvinyl alcohol solution (the addition amount of polyvinyl alcohol is 5% of the amount of the premixed powder in terms of mass percentage) into the sieved material, uniformly mixing, sieving the powder particles by using the 60-mesh standard sieve, and pressing the sieved material under the pressure of 200MPa to obtain a cylindrical green body with the diameter of 15mm and the thickness of 6-8 mm;
(8) rubber discharging: placing the cylindrical green body in a high-temperature furnace, heating to 600 ℃ at the speed of 3 ℃/min, and preserving heat for 3 h;
(9) and (3) sintering: sintering the cylindrical green body subjected to the binder removal treatment at about 1450 ℃ for 4 hours, and then cooling along with a furnace to obtain the microwave dielectric ceramic material 0.6CaxSr1-xTa2O6-0.4LaAlO3(x＝0.6)。
(10) And (3) later-stage mechanical processing: sintered 0.6CaxSr1-xTa2O6-0.4LaAlO3And (x is 0.6) grinding and polishing the ceramic to obtain a finished ceramic product with a flat and smooth surface. The bulk density of the ceramic samples was measured using the archimedes drainage method. Determining intermediate phases in the sintering process and final phases of reaction products by using an X-ray diffractometer (D/MAX 2000X), and continuously scanning at 1 degree/min, wherein the result shows that the main crystal phase of the ceramic is in an easily-decomposable stone structure, the ceramic forms a single-phase solid solution, and no second phase exists; the microwave dielectric property is tested by a vector network analyzer (Keysight E5232B); the microstructure morphology was observed using a white light interferometer (KLA-Tencor MicroXAM-800).
Example 2
This example provides a microwave dielectric ceramic material with a chemical composition of 0.6CaxSr1-xTa2O6-0.4LaAlO3(x ═ 0.7), the preparation method comprising the following steps:
(1) preparing materials: raw material SrCO3、CaCO3And Ta2O5As a raw material, in accordance with CaxSr1-xTa2O6(x is 0.7) in a stoichiometric ratio;
(2) mixing materials: mixing the materials obtained by proportioning, ball milling stones and purified water according to the proportion of 1: 3: 1.2, putting the mixture into a ball mill for wet ball milling (the rotating speed is about 150r/min), wherein the ball milling time is 20 hours, and obtaining slurry raw materials;
(3) drying: putting the slurry raw material in the step (2) into an oven to be dried to constant weight to obtain a dry mixture;
(4) pre-burning: sieving the mixture obtained in the step (3) with a 80-mesh sieve for dispersion, and then placing the mixture into a high-temperature furnace for presintering for 4 hours at the presintering temperature of 1150 ℃ to obtain CaxSr1-xTa2O6(x ═ 0.7) powder;
(5) ball milling: adding the Ca of the step (4) according to the stoichiometric ratioxSr1-xTa2O6Adding pure LaAlO into (x is 0.7) powder3Adding purified water, and grinding in a ball mill for 10h to form premixed slurry;
(6) drying: placing the premixed slurry obtained in the step (5) in an oven, and drying at 60 ℃ to constant weight to obtain premixed powder;
(7) and (3) granulation: sieving the premixed slurry obtained in the step (6) by using a 60-mesh standard sieve, adding a polyvinyl alcohol solution (the addition amount of polyvinyl alcohol is 5% of the amount of the premixed powder in terms of mass percentage) into the sieved material, uniformly mixing, sieving the powder particles by using the 60-mesh standard sieve, and pressing the sieved material under the pressure of 200MPa to obtain a cylindrical green body with the diameter of 15mm and the thickness of 6-8 mm;
(8) rubber discharging: placing the cylindrical green body in a high-temperature furnace, heating to 600 ℃ at the speed of 3 ℃/min, and preserving heat for 3 h;
(9) and (3) sintering: sintering the cylindrical green body subjected to the binder removal treatment at about 1450 ℃ for 4 hours, and then cooling along with a furnace to obtain the microwave dielectric ceramic material 0.6CaxSr1-xTa2O6-0.4LaAlO3(x＝0.7)。
(10) And (3) later-stage mechanical processing: sintered 0.6CaxSr1-xTa2O6-0.4LaAlO3And (x is 0.7) grinding and polishing the ceramic to obtain a finished ceramic product with a flat and smooth surface. The bulk density of the ceramic samples was measured using the archimedes drainage method. Determination of the mesophase during sintering by means of an X-ray diffractometer (D/MAX 2000X)And the final phase of the reaction product, a continuous scanning mode, 1 degree/min, results show that the main crystal phase of the ceramic is a structure of easy-to-dissolve stone, the ceramic forms a single-phase solid solution, and no second phase exists; the microwave dielectric property is tested by a vector network analyzer (Keysight E5232B); the microstructure morphology was observed using a white light interferometer (KLA-Tencor MicroXAM-800).
Example 3
This example provides a microwave dielectric ceramic material with a chemical composition of 0.6CaxSr1-xTa2O6-0.4LaAlO3(x ═ 0.8), the preparation method comprises the following steps:
(1) preparing materials: raw material SrCO3、CaCO3And Ta2O5As a raw material, in accordance with CaxSr1-xTa2O6(x is 0.8) in a stoichiometric ratio;
(2) mixing materials: mixing the materials obtained by proportioning, ball milling stones and purified water according to the proportion of 1: 3: 1.2, putting the mixture into a ball mill for wet ball milling (the rotating speed is about 150r/min), wherein the ball milling time is 20 hours, and obtaining slurry raw materials;
(3) drying: putting the slurry raw material in the step (2) into an oven to be dried to constant weight to obtain a dry mixture;
(4) pre-burning: sieving the mixture obtained in the step (3) with a 80-mesh sieve for dispersion, and then placing the mixture into a high-temperature furnace for presintering for 4 hours at the presintering temperature of 1150 ℃ to obtain CaxSr1-xTa2O6(x ═ 0.8) powder;
(5) ball milling: adding the Ca of the step (4) according to the stoichiometric ratioxSr1-xTa2O6Adding pure LaAlO into (x is 0.8) powder3Adding purified water, and grinding in a ball mill for 10h to form premixed slurry;
(6) drying: placing the premixed slurry obtained in the step (5) in an oven, and drying at 60 ℃ to constant weight to obtain premixed powder;
(7) and (3) granulation: sieving the premixed slurry obtained in the step (6) by using a 60-mesh standard sieve, adding a polyvinyl alcohol solution (the addition amount of polyvinyl alcohol is 5% of the amount of the premixed powder in terms of mass percentage) into the sieved material, uniformly mixing, sieving the powder particles by using the 60-mesh standard sieve, and pressing the sieved material under the pressure of 200MPa to obtain a cylindrical green body with the diameter of 15mm and the thickness of 6-8 mm;
(8) rubber discharging: placing the cylindrical green body in a high-temperature furnace, heating to 600 ℃ at the speed of 3 ℃/min, and preserving heat for 3 h;
(9) and (3) sintering: sintering the cylindrical green body subjected to the binder removal treatment at about 1450 ℃ for 4 hours, and then cooling along with a furnace to obtain the microwave dielectric ceramic material 0.6CaxSr1-xTa2O6-0.4LaAlO3(x＝0.8)。
(10) And (3) later-stage mechanical processing: sintered 0.6CaxSr1-xTa2O6-0.4LaAlO3And (x is 0.8) grinding and polishing the ceramic to obtain a finished ceramic product with a flat and smooth surface. The bulk density of the ceramic samples was measured using the archimedes drainage method. Determining intermediate phases in the sintering process and final phases of reaction products by using an X-ray diffractometer (D/MAX 2000X), and continuously scanning at 1 degree/min, wherein the result shows that the main crystal phase of the ceramic is in an easily-decomposable stone structure, the ceramic forms a single-phase solid solution, and no second phase exists; the microwave dielectric property is tested by a vector network analyzer (Keysight E5232B); the microstructure morphology was observed using a white light interferometer (KLA-Tencor MicroXAM-800).
Example 4
This example provides a microwave dielectric ceramic material with a chemical composition of 0.6CaxSr1-xTa2O6-0.4LaAlO3(x ═ 0.9), the preparation method comprising the following steps:
(1) preparing materials: raw material SrCO3、CaCO3And Ta2O5As a raw material, in accordance with CaxSr1-xTa2O6(x is 0.9) in a stoichiometric ratio;
(2) mixing materials: mixing the materials obtained by proportioning, ball milling stones and purified water according to the proportion of 1: 3: 1.2, putting the mixture into a ball mill for wet ball milling (the rotating speed is about 150r/min), wherein the ball milling time is 20 hours, and obtaining slurry raw materials;
(3) drying: putting the slurry raw material in the step (2) into an oven to be dried to constant weight to obtain a dry mixture;
(4) pre-burning: sieving the mixture obtained in the step (3) with a 80-mesh sieve for dispersion, and then placing the mixture into a high-temperature furnace for presintering for 4 hours at the presintering temperature of 1150 ℃ to obtain CaxSr1-xTa2O6(x ═ 0.9) powder;
(5) ball milling: adding the Ca of the step (4) according to the stoichiometric ratioxSr1-xTa2O6Adding pure LaAlO into (x is 0.9) powder3Adding purified water, and grinding in a ball mill for 10h to form premixed slurry;
(6) drying: placing the premixed slurry obtained in the step (5) in an oven, and drying at 60 ℃ to constant weight to obtain premixed powder;
(7) and (3) granulation: sieving the premixed slurry obtained in the step (6) by using a 60-mesh standard sieve, adding a polyvinyl alcohol solution (the addition amount of polyvinyl alcohol is 5% of the amount of the premixed powder in terms of mass percentage) into the sieved material, uniformly mixing, sieving the powder particles by using the 60-mesh standard sieve, and pressing the sieved material under the pressure of 200MPa to obtain a cylindrical green body with the diameter of 15mm and the thickness of 6-8 mm;
(8) rubber discharging: placing the cylindrical green body in a high-temperature furnace, heating to 600 ℃ at the speed of 3 ℃/min, and preserving heat for 3 h;
(9) and (3) sintering: sintering the cylindrical green body subjected to the binder removal treatment at about 1450 ℃ for 4 hours, and then cooling along with a furnace to obtain the microwave dielectric ceramic material 0.6CaxSr1-xTa2O6-0.4LaAlO3(x＝0.9)。
(10) And (3) later-stage mechanical processing: sintered 0.6CaxSr1-xTa2O6-0.4LaAlO3And (x is 0.9) grinding and polishing the ceramic to obtain a finished ceramic product with a flat and smooth surface. The bulk density of the ceramic samples was measured using the archimedes drainage method. Determining intermediate phases in the sintering process and final phases of reaction products by using an X-ray diffractometer (D/MAX 2000X), and continuously scanning at 1 degree/min, wherein the result shows that the main crystal phase of the ceramic is in an easily-decomposable stone structure, the ceramic forms a single-phase solid solution, and no second phase exists; the microwave dielectric property is tested by a vector network analyzer (Keysight E5232B);the microstructure morphology was observed using a white light interferometer (KLA-Tencor MicroXAM-800).
Comparative example 1
Basically, the method is the same as the method in example 4, and only differs from the method in that: x is 0.5.
Comparative example 2
Basically, the method is the same as the method in example 4, and only differs from the method in that: the sintering temperature in step (9) was 1400 ℃.
Comparative example 3
Basically, the method is the same as the method in example 4, and only differs from the method in that: the sintering temperature in step (9) was 1500 ℃.
Performance testing
The microwave dielectric properties of the microwave dielectric ceramics obtained in the above examples 1 to 4 and comparative examples 1 to 3 were measured by using a Keysight E5232B vector network analyzer at the resonance frequency of the cylindrical ceramics, as shown in Table 1 below (dielectric constant measuring System (dielectric resonator method)), in which a measuring jig was connected to the vector network analyzer by a cable, the measuring jig was placed in a high-low temperature chamber, the resonance frequency, Q x F value and dielectric constant at room temperature were measured at room temperature, and then the temperature was raised to 125 ℃ to measure the resonance frequency at that time, and the temperature coefficient of resonance frequency, τ, was calculated at that timef)：
TABLE 1
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
Claims (10)
1. A microwave dielectric ceramic material is characterized by comprising the following chemical components: 0.6CaxSr1-xTa2O6-0.4LaAlO3And x is 0.6 or more and 0.9 or less.
2. A microwave dielectric ceramic material according to claim 1 wherein x is 0.8 or greater and 0.9 or less.
3. The microwave dielectric ceramic material as claimed in claim 1, wherein the sintering temperature of the microwave dielectric ceramic material is 1440-1460 ℃.
4. The microwave dielectric ceramic material as claimed in claim 1, wherein the dielectric constant r of the microwave dielectric ceramic material is 19.43-25.22, the quality factor Qxf is 100232-124564 GHz, and the temperature coefficient τ f of the resonance frequency is-16.3-1.5 ppm/° C.
5. A method for preparing a microwave dielectric ceramic material as claimed in any one of claims 1 to 4, wherein the method comprises the following steps:
(1) with SrCO3、CaCO3And Ta2O5As a raw material, in accordance with CaxSr1-xTa2O6The formula is prepared according to the stoichiometric ratio of (A), x is more than or equal to 0.6 and less than or equal to 0.9;
(2) performing wet ball milling on the material prepared in the step (1) to obtain slurry-like material;
(3) drying the slurry-like material prepared in the step (2) to constant weight to obtain a dry mixture;
(4) sieving the mixture prepared in the step (3), and pre-sintering at 1110-1180 ℃ to prepare CaxSr1-xTa2O6Powder, x is more than or equal to 0.6 and less than or equal to 0.9;
(5) LaAlO is added according to the stoichiometric ratio3Adding the Ca prepared in the step (4)xSr1-xTa2O6Performing wet ball milling on the powder to obtain premixed slurry;
(6) drying the premixed material prepared in the step (5) to constant weight to obtain premixed powder;
(7) sieving the premixed powder in the step (6), and mixing the sieved material with a binder to prepare a green body;
(8) placing the green body prepared in the step (7) in a high-temperature furnace, heating to 580-620 ℃ at the speed of 2.5-3.5 ℃/min, and preserving heat for 2.5-3.5 h;
(9) sintering the green body treated in the step (8) at 1440-1460 ℃ to obtain the microwave dielectric ceramic material with the following chemical components: 0.6CaxSr1-xTa2O6-0.4LaAlO3And x is 0.6 or more and 0.9 or less.
6. A preparation method of a microwave dielectric ceramic material as claimed in claim 5, wherein in the step (2), the wet ball milling is performed by using the materials prepared in the step (1), ball milling stones and water according to a mass ratio of 1: 2-4: 1.0-1.4.
7. A preparation method of a microwave dielectric ceramic material as claimed in claim 1, wherein in the step (2) and the step (5), the ball mill adopted by the wet ball milling is a planetary ball mill, and the set rotating speed is 110r/min-180 r/min.
8. The preparation method of the microwave dielectric ceramic material as claimed in claim 1, wherein in the step (7), the binder is polyvinyl alcohol, the polyvinyl alcohol is added in the form of an aqueous solution of polyvinyl alcohol, and the addition amount of the polyvinyl alcohol is 2-8% of the material sieved out from the premixed powder in percentage by mass.
9. The method for preparing microwave dielectric ceramic material according to claim 1, wherein in step (9), the sintering process comprises: heating to 1440-1460 ℃ at a speed of 2.5-3.5 ℃/min.
10. Use of a microwave dielectric ceramic material according to any one of claims 1 to 4 in the manufacture of a microwave device.
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